Hydrochloric Acid → HCID 21289929, compound

HRID 867535Notes

Reaction equation

HRID 867535 reaction equation
[Cl:1][C:2]1[C:7]2[C:8](=[O:21])[NH:9][CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([O:18]CC)=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1.[OH-].[Na+].C(O)C.Cl>O>[Cl:1][C:2]1[C:7]2[C:8](=[O:21])[NH:9][CH2:10][C:11]3[N:12]([CH:13]=[N:14][C:15]=3[C:16]([OH:18])=[O:17])[C:6]=2[CH:5]=[CH:4][CH:3]=1

Participants

6

Reactant 4

HCID 313Hydrochloric AcidHCID 702EthanolHCID 14798Sodium HydroxideHCID 21289921HCID 21289921, compound

Product 1

HCID 21289929HCID 21289929, compound

Reagents, catalysts & solvents 1

HCID 962WaterSolvent2×

Procedure

A mixture of 9 g (29.4 mmol) of ethyl 7-chloro-5,6-dihydro-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylate, 1.434 g (35.9 mmol) of sodium hydroxide, 30 ml of ethanol and 15 ml of water is heated to boiling under reflux for 70 minutes. The mixture is then diluted with 80 ml of water, filtered, the filtrate is neutralized by the addition of 8.9 ml (35.9 mmol) of 4N hydrochloric acid and the ethanol is distilled off in vacuo. The residue is subsequently cooled to about 0°, the product is filtered off under suction, rinsed with water and dried at 80°-90° in a high vacuum. There is obtained 7-chloro-5,6-dihydro-6-oxo-4H-imidazo[1,5-a][1,4]benzodiazepine-3-carboxylic acid of decomposition point 289°.

Workup

  1. temperatureis heated
  2. temperatureunder reflux for 70 minutes
  3. filtrationfiltered
  4. distillationthe ethanol is distilled off in vacuo
  5. temperatureThe residue is subsequently cooled to about 0°
  6. filtrationthe product is filtered off under suction
  7. washrinsed with water
  8. customdried at 80°-90° in a high vacuum

Sources & evidence

ORD record
ord-65bdbf486262459e9755369681813402
Source dataset
uspto-grants-1988_10
Patent number
US04775671

Reaction notes

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